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任呼博, 别振英, 朱友, 等. 超高效液相色谱法同时测定烟用香精料液中的糠醛、5-羟甲基糠醛与5-甲基糠醛[J]. 分析测试学报, 2015,34(11):1291-1295.
Simultaneous Determination of Furfural,5-Hydroxymethylfurfural and 5-Methylfurfural in Cigarette Fragrances by Ultra-high Performance Liquid Chromatography[J]. 2015,34(11):1291-1295.
建立了同时测定烟用香精料液中糠醛、5-羟甲基糠醛和5-甲基糠醛的超高效液相色谱(UPLC)方法。样品经流动相稀释、振荡、过滤后,采用C18(2.1 mm i.d.×100 mm,1.7 μm)柱,以乙腈-水(10∶90)为流动相,在流速0.3 mL/min条件下等度洗脱分离,以二极管阵列检测器在波长280 nm下检测,外标法定量。该方法5 min内即可实现3种目标物的分离,5-羟甲基糠醛、糠醛和5-甲基糠醛的线性范围分别为0.004 2~40.00 mg/kg,0.004 6~30.00 mg/kg,0.006 9~30.00 mg/kg;相关系数(r2)分别为0.999 2,0.999 9和0.999 8;检出限(S/N=3)分别为1.24,1.37,2.06 μg/kg;相对标准偏差(RSD,n=11)为0.1%~0.4%;加标水平为0.005 0~10.18 mg/kg时,3种化合物的回收率为91.7%~106.0%。该方法操作简便、分析快速、结果准确,适用于烟用香精料液中5-羟甲基糠醛、糠醛和5-甲基糠醛的检测。
An ultra-high performance liquid chromatographic(UPLC)method for the simultaneous determination of furfural,5-hydroxymethylfurfural and 5-methylfurfural in cigarette fragrances was established.After dilution,vibration and filtration,the cigarette additives were separated on a C18(2.1 mm i.d.× 100 mm,1.7 μm) column under isocratic elution mode using acetonitrile-water(10∶90) as mobile phase at a flow rate of 0.3 mL/min.The quantification of these analytes was achieved by the external standard method with a diode-array detector at 280 nm.Baseline separation of these analytes was achieved within 5.0 min.The linear ranges for 5-hydroxymethylfurfural,furfural and 5-methylfurfural were in the ranges of 0.004 2-40.00 mg/kg,0.004 6-30.00 mg/kg,0.006 9-30.00 mg/kg,with correlation coefficients(r2) of 0.999 2,0.999 9 and 0.999 8,respectively.The detection limits(S/N=3) for three analytes were 1.24,1.37,2.06 μg/kg,respectively.Relative standard deviations(RSD,n=11) were in the range of 0.1%-0.4%.The recoveries at spiked concentration of 0.005 0-10.18 mg/kg were 91.7%-106.0%.The proposed method has the merits of easy operation,fast analysis and accurate results,and is suitable for the simultaneous determination of 5-hydroxymethylfurfural,furfural and 5-methylfurfural in cigarette fragrances.
超高效液相色谱法(UPLC)烟用香精料液糠醛5-羟甲基糠醛5-甲基糠醛
ultra-high performance liquid chromatography(UPLC)cigarette fragrancesfurfural5-hydroxymethylfurfural5-methylfurfural
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